CN207512313U - A kind of indium phosphide single crystal controlled growth device - Google Patents
A kind of indium phosphide single crystal controlled growth device Download PDFInfo
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- CN207512313U CN207512313U CN201721640945.5U CN201721640945U CN207512313U CN 207512313 U CN207512313 U CN 207512313U CN 201721640945 U CN201721640945 U CN 201721640945U CN 207512313 U CN207512313 U CN 207512313U
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- ampoule
- indium phosphide
- single crystal
- phosphide single
- growth device
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Abstract
The utility model is related to a kind of indium phosphide single crystal controlled growth device, including enclosed high pressure chamber, the heating furnace chamber mounted on enclosed high pressure intracavitary, ampoule support base, quartz ampoule, PBN crucibles and quartz cap；Heating furnace chamber is fixed on the inside of enclosed high pressure chamber, ampoule support base is arranged on the lower inside of heating furnace chamber, quartz ampoule is arranged on ampoule support base upper end, PBN crucibles are removably disposed in the inside of quartz ampoule, and quartz cap is arranged on the upper end of PBN crucibles and the space of sealing is surrounded with PBN crucibles；The central axial of ampoule support base upper end is provided with a heating tube, and the lower end cooperation of quartz ampoule is put in heating tube.The utility model can reduce solid liquid interface curvature and thermal stress in indium phosphide single crystal growth course, and the temperature gradient of indium phosphide single crystal growth course can be controlled.
Description
Technical field
The utility model is related to technical field of crystal growth, more particularly to a kind of indium phosphide single crystal controlled growth device.
Background technology
Major diameter low-dislocation-density indium phosphide single crystal growth at present mainly uses vertical gradient freeze technique (VGF methods).
In order to obtain the indium phosphide single crystal of high quality, low dislocation, temperature gradient, solid-liquid interface shape and the thermal stress of growth course etc.
Factors influence crystal forming rate and into crystalloid amount, the accurate control of the crystal growth rate in being in particular in crystal growth technique excessively
System.Usual VGF method indium phosphide crystal growers are in one built in high-pressure chamber round straight tube shape heating furnace chamber, and heating furnace chamber is set
Several heating zones control each warm area temperature, reach a suitable crystal growth gradient to obtain required growth rate
Complete the growth of crystal.The growing method of crystal is that indium phosphide polycrystal material is packed into a PBN crucible with taper, is encapsulated in one
In a quartz ampoule to match with PBN crucibles, it is placed in heating and melting in round straight tube shape heating furnace chamber, growth.
In the prior art, for the PBN crucibles of major diameter grow indium phosphide single crystal, due to PBN crucibles conical section away from
Heater strip from circle straight tube shape heating furnace chamber, which does not wait, causes the radial and axial temperature gradient of conical section to become much larger, growth course
Solid liquid interface curvature and thermal stress also accordingly become larger.Moreover, PBN crucibles because its material a, c direction (a be perpendicular to crucible
Direction, c are along sidewall of crucible direction) thermal conductivity difference (a:0.25cal/cm·s·℃,c:0.04cal/cms DEG C) spy
Property, nearby a large amount of hot-fluid are guided grain boundary by sidewall of crucible, and crystal edge forms larger degree of supercooling, makes the life needed for crystal
The defects of long interface stability is deteriorated, and growth rate is difficult to control, also easily causes the polycrystalline, twin, dislocation of crystal growth, directly
Influence crystal forming rate and into crystalloid amount.
Utility model content
Based on this, the purpose of the utility model is to overcome the deficiencies in the prior art, and it is controlled to provide a kind of indium phosphide single crystal
Grower, the device can reduce solid liquid interface curvature and thermal stress in indium phosphide single crystal growth course, and indium phosphide
The temperature gradient of single crystal growth process can be controlled.
To achieve these goals, the technical solution adopted in the utility model is：
A kind of indium phosphide single crystal controlled growth device, including enclosed high pressure chamber, the heating furnace mounted on enclosed high pressure intracavitary
Chamber, ampoule support base, quartz ampoule, PBN crucibles and quartz cap；Heating furnace chamber is fixed on the inside of enclosed high pressure chamber,
Ampoule support base is arranged on the lower inside of heating furnace chamber, and quartz ampoule is arranged on ampoule support base upper end, and PBN crucibles are detachable
Ground is arranged on the inside of quartz ampoule, and quartz cap is arranged on the upper end of PBN crucibles and the space of sealing is surrounded with PBN crucibles；Peace
The central axial of small jar support base upper end is provided with a heating tube, and the lower end cooperation of quartz ampoule is put in heating tube.
Indium phosphide single crystal controlled growth device described in the utility model as a result, is set using ampoule support base is central axial
A V-type heating tube is put, can effectively and efficiently and easily reduce axially and radially temperature gradient, and heat by V-type
The radial direction heat leakage for rising heat radiation compensation PBN sidewall of crucible edge crystal of pipe；Reduce 1/ than common VGF stoves axial-temperature gradient
3rd, radial symmetry gradient reduces 2/3；The solid liquid interface curvature and thermal stress of crystal growing process become smaller and solid liquid interface it is steady
Qualitative to greatly improve, crystal growth rate is controlled, the defects of considerably reducing the polycrystalline, twin, dislocation of crystal growth,
Therefore high crystal forming rate is obtained and into crystalloid amount.
Further, the heating tube is V-type heating tube.
Further, the quartz ampoule includes sequentially connected long cylinder, ampoule centrum and ampoule seed crystal well, ampoule
The upper port diameter of centrum is equal to the lower port diameter of long cylinder, and the lower port diameter of ampoule centrum is equal to the upper of ampoule seed crystal well
Port diameter, and the diameter of ampoule centrum is gradually reduced from upper port along lower port direction.
Further, the upper port diameter of the V-type heating tube is equal to 3/5ths, V of ampoule centrum upper port diameter
The lower port diameter of type heating tube is equal to 1/5th of ampoule centrum upper port diameter.
Further, the upper port plane of the V-type heating tube is parallel with the upper port plane of ampoule seed crystal well.
Further, the V-type heating tube includes vitreosil pipe and more high temperature resistance silks, more high temperature resistance silks
It is uniformly outer to be wound on the lateral surface of quartz ampoule.
Further, uniformly filled with low-density insulation alumina silicate ceramic fiber cotton in the V-type heating tube.
Further, low-density insulating oxide zircon ceramic cellucotton is uniformly filled with outside the more high temperature resistance silks.
Further, the more high temperature resistance silks are evenly arranged in V-type heating infratubal port and extremely divide apart from upper port three
Two lateral surface on.
Further, the more high temperature resistance silks are additionally provided with a temperature-control heat couple.
Description of the drawings
Fig. 1 is the structure diagram of the indium phosphide single crystal controlled growth device of the utility model；
Fig. 2 is the structure diagram of quartz ampoule shown in FIG. 1.
Specific embodiment
To further illustrate each embodiment, the utility model is provided with attached drawing.These attached drawings is in the utility model exposure
A part for appearance mainly to illustrate embodiment, and can coordinate the associated description of specification to explain the running of embodiment original
Reason.Cooperation will be understood that other may obtain embodiment and this practicality with reference to these contents, those of ordinary skill in the art
The advantages of novel.
It please refers to Fig.1 and Fig. 2, wherein, Fig. 1 is the structural representation of the indium phosphide single crystal controlled growth device of the utility model
Figure；Fig. 2 is the structure diagram of quartz ampoule shown in FIG. 1.
The indium phosphide single crystal controlled growth device of the utility model, including enclosed high pressure chamber 10, mounted on enclosed high pressure chamber
Heating furnace chamber 20, ampoule support base 30, quartz ampoule 40, PBN crucibles 50 and quartz cap 60 in 10；Heating furnace chamber 20 is installed
The inside of enclosed high pressure chamber 10 is fixed on, ampoule support base 30 is arranged on the lower inside of heating furnace chamber 20, and quartz ampoule 40 is set
It puts in 30 upper end of ampoule support base, PBN crucibles 50 are removably disposed in the inside of quartz ampoule 40, and quartz cap 60 is arranged on
The upper end of PBN crucibles 50 and the space that sealing is surrounded with PBN crucibles 50；The central axial of 30 upper end of ampoule support base is provided with one
Heating tube, the lower end cooperation of quartz ampoule 40 are put in heating tube.
Specifically, the heating tube is V-type heating tube 70, which includes vitreosil pipe 71 and more
High temperature resistance silk 72, more high temperature resistance silks 72 are uniformly outer to be wound on the lateral surface of quartz ampoule 71.Wherein, the V-type of the present embodiment
The electric thermal power of heating tube 70 is controlled by external PID temperature controls.
In the present embodiment, the quartz ampoule 40 includes sequentially connected long cylinder 41, ampoule centrum 42 and ampoule seed
Brilliant well 43, the upper port diameter of ampoule centrum 42 are equal to the lower port diameter of long cylinder 41, the lower port diameter of ampoule centrum 42
Equal to the upper port diameter of ampoule seed crystal well 43, and the diameter of ampoule centrum 42 is gradually reduced from upper port along lower port direction.
The upper port diameter of the V-type heating tube 70 is equal to 3/5ths of 42 upper port diameter of ampoule centrum, V-type heating
The lower port diameter of pipe 70 is equal to 1/5th of 42 upper port diameter of ampoule centrum.In addition, the upper end of the V-type heating tube 70
Mouth plane is parallel with the upper port plane of ampoule seed crystal well 43.
In the present embodiment, it is preferable that uniformly filled with low-density insulation alumina-silicate ceramic fibre in the V-type heating tube 70
Cotton 80.Also, low-density insulating oxide zircon ceramic cellucotton 90 is uniformly filled with outside the more high temperature resistance silks 72.
The more high temperature resistance silks 72 are evenly arranged in 70 lower port of V-type heating tube to apart from upper port 2/3rds
On lateral surface.In addition, the more high temperature resistance silks 72 are additionally provided with a temperature-control heat couple.
Wherein, the heating furnace chamber 20 is circle straight tube shape heating furnace chamber, and heating furnace chamber 20 is sequentially distributed from top to bottom
There are the first warm area, the second warm area, third warm area and four-temperature region.Wherein, the middle lower end of V-type heating tube 70 is to ampoule support base
30 bottom is the first warm area, and the lower port plane of the long cylinder 41 of the middle lower end of V-type heating tube 70 to quartz ampoule 40 is the
Two warm areas, the upper port plane of the long cylinder 41 of the lower port plane of the long cylinder 41 of quartz ampoule 40 to quartz ampoule 40 are the
Three-temperature-zone, upper port plane to the top of heating furnace chamber 20 of the long cylinder 41 of quartz ampoule 40 is four-temperature region.
Illustrate the operation principle of the indium phosphide single crystal controlled growth device of the utility model below：
Polycrystal material, proportioning red phosphorus, boron oxide loading have been placed in the PBN crucibles 50 of seed crystal first.
Then above-mentioned charged PBN crucibles 50 are moved into matched quartz ampoule 40, is put into sealing quartz cap 60, takes out
Vacuum, with oxyhydrogen flame sealing.
The quartz ampoule 40 sealed vertically is put into round straight tube shape heating furnace chamber 20 again, 40 top of sealing quartz ampoule,
Then enclosed high pressure chamber 10 is sealed again.
Finally check water, electricity and gas connection, increasing temperature and pressure controls each Heating Zone Temperature, melts polycrystal material in advance, keeps the temperature
Then certain time starts V-type heating tube 70 and heats, adjust axial radial temperature and 50 taper temperature of PBN crucibles ladder between warm area
Degree, starts to cool down by program after connecting seed crystal, crystal from bottom to top solidification and crystallization, until completing the life of entire indium phosphide single crystal body
It is long.
Wherein, when polycrystal material, which heats up, to be melted, the electric thermal power of V-type heating tube 70 is adjusted, it is axial to reduce heating furnace chamber 20
And radial symmetry gradient, heat in entire heating furnace chamber 20 is made to tend to be uniform and stable, polycrystal material fusing homogenieity further improves；
Start to connect seed crystal after seeding temperature reaches, adjust the electric thermal power of V-type heating tube 70, reduce the axial direction and diameter of crystal and melt
To temperature gradient, make to connect fisheye position and the adjustment of solid liquid interface curvature；When crystal growth, the electric heating of V-type heating tube 70 is adjusted
Power compensates the radial direction heat leakage of crystal, maintains the stability of solid liquid interface, and crystal growth turn/shouldering process is made accurately to adjust
Growth rate, the polycrystalline for inhibiting the boundary effect of 50 wall edge crystal growth of PBN crucibles and generating, twinning.
In addition, the utility model specifically provides two different high quality indium phosphide single crystal growth preparing methods：
The first is to mix 4 inches of indium phosphide single crystal body growth preparing methods of sulphur：By 4.5Kg indium phosphide polycrystals material and 0.6g
Indium sulfide, 72g waterless boron oxides, 48g red phosphorus are placed in the PBN crucibles 50 for having placed seed crystal, are pushed into quartz ampoule 40, vacuum
Welded seal quartz ampoule 40 is vertically put into enclosed high pressure chamber 10.Increasing temperature and pressure, control three or four area's temperature be 1070 DEG C, one
1010 DEG C of 2nd area temperature starting control, after melting duration 8h, starts V-type heating tube 70 and heats, and adjusts axial temperature between two, three-temperature-zone
Gradient 20 DEG C of axial-temperature gradient of control is spent, until the control of seed crystal point temperature is connect 1-2 DEG C on indium phosphide fusing point (1062 DEG C), PBN
50 tapered zone axial-temperature gradient control of crucible starts main cooling process after 3.5-4 °/cm, holding 6h, and crystal growth rate is protected
It holds in 0.6mm/h.Take out crystal ingot after EP (end of program), crystal ingot equal-diameter part length 90mm, crystal forming rate 70%, appearance after hcl corrosion
Without crystal defect presence is evident that, seed crystal fusing length 8mm, liquid-solid boundary interface is smooth, 4 inches of crystal ingot tail portion cutting sheet
EPD is 150/cm2.
This preparation method reduces relative to the indium phosphide single crystal ingot EPD (500-800/cm2) that common VGF stoves are grown
2/3, crystal forming rate improves 30%.
Second is to mix 4 inches of indium phosphide single crystal body growths of iron：By 4.5Kg indium phosphide polycrystals material and 1.45g fes,
90g waterless boron oxides, 58g red phosphorus are placed in the PBN crucibles for having placed seed crystal, are pushed into quartz ampoule 40, vacuum welding sealing
Quartz ampoule 40 is vertically put into enclosed high pressure chamber 10.Increasing temperature and pressure, three or four area's temperature of control are 1075 DEG C, one or two area's temperature
1020 DEG C of starting control after melting duration 12h, starts V-type heating tube 70 and heats, adjust axial-temperature gradient between two, three-temperature-zone
25 DEG C of axial-temperature gradient is controlled, until the control of seed crystal point temperature is connect 1-2 DEG C on indium phosphide fusing point (1062 DEG C), PBN crucibles 50
Tapered zone axial-temperature gradient control is in 4-5 °/cm, and holding starts main cooling process after 6 hours, and crystal growth rate is maintained at
0.4mm/h.Take out crystal ingot after EP (end of program), crystal ingot equal-diameter part length 90mm, crystal forming rate 60%, appearance is without bright after hcl corrosion
Aobvious visible crystal defect exists, and seed crystal fusing length 12mm, liquid-solid boundary interface is smooth, 4 inches of crystal ingot tail portion cutting sheet EPD
For 500/cm2.
This preparation method mixes iron monocrystal ingot EPD (1000-1200/cm2) relative to the indium phosphide that common VGF stoves are grown
Reduce 1/2, crystal forming rate improves 20%.
Compared with prior art, the indium phosphide single crystal controlled growth device of the utility model, utilizes ampoule support base center
One V-type heating tube of axial setting, can effectively and efficiently and easily reduce axially and radially temperature gradient, and pass through V
The radial direction heat leakage for rising heat radiation compensation PBN sidewall of crucible edge crystal of type heating tube；Than common VGF stoves axial-temperature gradient
Reduce 1/3, radial symmetry gradient and reduce 2/3；The solid liquid interface curvature and thermal stress of crystal growing process become smaller and solid-liquid circle
The stability in face greatly improves, and crystal growth rate is controlled, and considerably reduces the polycrystalline, twin, dislocation of crystal growth
The defects of, therefore to obtain high crystal forming rate and into crystalloid amount.
Embodiment described above only expresses the several embodiments of the utility model, and description is more specific and detailed,
But therefore it can not be interpreted as the limitation to utility model patent range.It should be pointed out that the common skill for this field
For art personnel, without departing from the concept of the premise utility, various modifications and improvements can be made, these are belonged to
The scope of protection of the utility model.
Claims (10)
1. a kind of indium phosphide single crystal controlled growth device, including enclosed high pressure chamber, mounted on enclosed high pressure intracavitary heating furnace chamber,
Ampoule support base, quartz ampoule, PBN crucibles and quartz cap；It is characterized in that：Heating furnace chamber is fixed on enclosed high pressure chamber
Inside, ampoule support base is arranged on the lower inside of heating furnace chamber, and quartz ampoule is arranged on ampoule support base upper end, PBN earthenwares
Crucible is removably disposed in the inside of quartz ampoule, and quartz cap is arranged on the upper end of PBN crucibles and surrounds sealing with PBN crucibles
Space；The central axial of ampoule support base upper end is provided with a heating tube, and the lower end cooperation of quartz ampoule is put in heating tube.
2. indium phosphide single crystal controlled growth device according to claim 1, it is characterised in that：The heating tube adds for V-type
Heat pipe.
3. indium phosphide single crystal controlled growth device according to claim 2, it is characterised in that：The quartz ampoule include according to
Long cylinder, ampoule centrum and the ampoule seed crystal well of secondary connection, the upper port diameter of ampoule centrum are equal to the lower port of long cylinder
Diameter, the lower port diameter of ampoule centrum are equal to the upper port diameter of ampoule seed crystal well, and the diameter of ampoule centrum is from upper port
It is gradually reduced along lower port direction.
4. indium phosphide single crystal controlled growth device according to claim 3, it is characterised in that：The V-type heating tube it is upper
Port diameter is equal to 3/5ths of ampoule centrum upper port diameter, and the lower port diameter of V-type heating tube is equal on ampoule centrum
/ 5th of port diameter.
5. indium phosphide single crystal controlled growth device according to claim 3, it is characterised in that：The V-type heating tube it is upper
Port plane is parallel with the upper port plane of ampoule seed crystal well.
6. according to claim 2 to 5 any one of them indium phosphide single crystal controlled growth device, it is characterised in that：The V-type adds
Heat pipe includes vitreosil pipe and more high temperature resistance silks, and more high temperature resistance silks are uniformly wound on the lateral surface of quartz ampoule outside
On.
7. indium phosphide single crystal controlled growth device according to claim 6, it is characterised in that：In the V-type heating tube
It is even to be filled with low-density insulation alumina silicate ceramic fiber cotton.
8. indium phosphide single crystal controlled growth device according to claim 7, it is characterised in that：The more high temperature resistance silks
It is outer to be uniformly filled with low-density insulating oxide zircon ceramic cellucotton.
9. indium phosphide single crystal controlled growth device according to claim 8, it is characterised in that：The more high temperature resistance silks
It is evenly arranged on V-type heating infratubal port to the lateral surface apart from upper port 2/3rds.
10. indium phosphide single crystal controlled growth device according to claim 9, it is characterised in that：The more high temperature resistances
Silk is additionally provided with a temperature-control heat couple.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201721640945.5U CN207512313U (en) | 2017-11-30 | 2017-11-30 | A kind of indium phosphide single crystal controlled growth device |
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| CN201721640945.5U CN207512313U (en) | 2017-11-30 | 2017-11-30 | A kind of indium phosphide single crystal controlled growth device |
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| CN201721640945.5U Expired - Fee Related CN207512313U (en) | 2017-11-30 | 2017-11-30 | A kind of indium phosphide single crystal controlled growth device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110512274A (en) * | 2019-09-30 | 2019-11-29 | 山西中科晶电信息材料有限公司 | A kind of device of the reduction GaAs crystal twin based on VGF method |
| WO2020118999A1 (en) * | 2018-12-14 | 2020-06-18 | 中国电子科技集团公司第十三研究所 | Quartz tube and device for crystal growth by vb/vgf method |
| CN112760713A (en) * | 2020-12-28 | 2021-05-07 | 中锗科技有限公司 | Crucible for InP crystal growth and InP crystal growth method |
| CN113512754A (en) * | 2021-05-26 | 2021-10-19 | 中锗科技有限公司 | Alumina ceramic crucible, use structure thereof and method for growing single crystal |
| CN113774489A (en) * | 2021-07-30 | 2021-12-10 | 合肥天曜新材料科技有限公司 | Growth device and growth method of indium phosphide single crystal |
| WO2024012520A1 (en) * | 2022-07-15 | 2024-01-18 | 中国电子科技集团公司第十三研究所 | Device and method for centrifugally synthesizing and growing compound crystal |
| CN117568915A (en) * | 2023-10-20 | 2024-02-20 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Controllable indium phosphide monocrystal growth device and growth method |
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- 2017-11-30 CN CN201721640945.5U patent/CN207512313U/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020118999A1 (en) * | 2018-12-14 | 2020-06-18 | 中国电子科技集团公司第十三研究所 | Quartz tube and device for crystal growth by vb/vgf method |
| CN110512274A (en) * | 2019-09-30 | 2019-11-29 | 山西中科晶电信息材料有限公司 | A kind of device of the reduction GaAs crystal twin based on VGF method |
| CN112760713A (en) * | 2020-12-28 | 2021-05-07 | 中锗科技有限公司 | Crucible for InP crystal growth and InP crystal growth method |
| CN113512754A (en) * | 2021-05-26 | 2021-10-19 | 中锗科技有限公司 | Alumina ceramic crucible, use structure thereof and method for growing single crystal |
| CN113774489A (en) * | 2021-07-30 | 2021-12-10 | 合肥天曜新材料科技有限公司 | Growth device and growth method of indium phosphide single crystal |
| WO2024012520A1 (en) * | 2022-07-15 | 2024-01-18 | 中国电子科技集团公司第十三研究所 | Device and method for centrifugally synthesizing and growing compound crystal |
| CN117568915A (en) * | 2023-10-20 | 2024-02-20 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Controllable indium phosphide monocrystal growth device and growth method |
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